CN113754436B - Preparation method of nanocrystalline laser-grade sesquioxide transparent ceramic - Google Patents
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Abstract
The invention discloses a nanocrystalline laserA process for preparing optical sesqui oxide transparent ceramic includes such steps as preparing Y 2 O 3 And a Cr-containing dopant of the formula (Cr) x Y 1‑x ) 2 O 3 Weighing and mixing to obtain mixed powder, wherein x is more than or equal to 0.0002 and less than or equal to 0.02, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Cr, Y 2 O 3 Powder; mixing Cr with Y 2 O 3 Molding the powder to obtain a blank; sintering the blank in a vacuum environment at 1200-1600 deg.C for 0.5-50h, hot isostatic pressing in an inert gas at 1200-1600 deg.C for 0.5-8h, annealing in air, oxygen or reducing atmosphere at 1100-1500 deg.C for 0.5-30h, and fine polishing two surfaces to obtain Cr, Y 2 O 3 The invention discloses a transparent ceramic, which takes a proper amount of Cr as a doping agent, can reduce the sintering temperature of pure sesquioxide ceramic, and can ensure that the prepared ceramic material has nano-scale grain size and laser-level transparency, and has excellent mechanical properties and infrared transmittance.
Description
Technical Field
The invention relates to a preparation method of a nanocrystalline laser-grade sesquioxide transparent ceramic, belonging to the technical field of sesquioxide transparent ceramics.
Background
Compared withCommon YAG materials, sesquioxide materials (e.g. Y) 2 O 3 、Sc 2 O 3 And Lu 2 O 3 ) Has lower phonon energy, lower thermal expansion coefficient and higher thermal conductivity, and has great development potential in the field of high-power solid laser. However, the melting point of sesquioxide is as high as 2400 ℃ or higher, and the transformation point is lower than the melting point, so that the technique of growing a single crystal thereof is extremely complicated. Furthermore, the size of the single crystal is limited by the equipment required and the mechanical properties are low, making it difficult to meet different applications. By adopting the ceramic preparation process, the sesquioxide transparent ceramic can be sintered at a temperature far lower than the melting point of the material, and the large-size, large-scale and low-cost preparation can be realized more easily. Meanwhile, the sesquioxide ceramic also has the characteristics of wide light transmission range, high mechanical strength, high refractoriness and high dielectric constant, can be used for manufacturing materials such as infrared windows, infrared fairings, high-temperature lenses, microwave substrates and the like, and has great application prospects in the civil and military fields.
For a high-power laser system, the good mechanical property can enable the material to bear more thermal stress, so that the damage of the material is avoided as much as possible, and the power scaling and amplification are facilitated; in addition to the basic requirement that the material has high infrared transmittance, the biggest challenge is to further improve the bending resistance. By means of the Hall-Petrc formula (sigma ∞ 1/d) 1/2 ) It is known that the grain size d is inversely proportional to the strength σ of the ceramic, i.e., the smaller the grain size, the higher the strength of the ceramic. In addition, according to the report of h. Yagi et al, since the crystal grains in the polycrystalline ceramic material are randomly oriented, a smaller crystal grain size may contribute to the elimination of internal stress of the ceramic.
Therefore, to improve the mechanical properties of the sesquioxide ceramics, it is critical that the ceramics have a smaller grain size while ensuring high optical quality. Dopants are typically added to the matrix material to lower the sintering temperature or to suppress grain boundary mobility, thereby reducing the grain size. In 2015, L, zhang et al with ZrO2 and La 2 O 3 Preparing Cr to Y as sintering aid by vacuum sintering 2 O 3 Transparent ceramics, discoveryThe incorporation of a suitable amount of Cr is beneficial for reducing the grain size and is considered to be a potential laser material with good mechanical properties. However, the Cr to Y produced 2 O 3 The grain size of the ceramic is large (8.3-4.3 μm for Cr doping concentrations of 0-0.7 at.%), and the feature of Cr doped sesquioxide ceramics that can be densified at low temperatures has not been found. The crystal material doped with Cr or co-doped with other rare earth ions (such as Yb3+, nd3+, and the like) is often used as a saturable absorber or a laser gain medium, and can improve the flash lamp pumping efficiency of the laser crystal material. Therefore, the further research on the Cr-doped sesquioxide transparent ceramic material has very important significance.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art that is already known to a person skilled in the art.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a nanocrystalline laser-grade sesquioxide transparent ceramic to solve the problem that the Cr: Y prepared in the prior art is 2 O 3 The grain size of the ceramic is large.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of nanocrystalline laser-grade sesquioxide transparent ceramics comprises the following steps: step A, adding Y 2 O 3 And a Cr-containing dopant of the formula (Cr) x Y 1-x ) 2 O 3 Weighing and mixing to obtain mixed powder, wherein x is more than or equal to 0.0002 and less than or equal to 0.02, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Cr, Y 2 O 3 Powder;
step B, mixing Cr and Y 2 O 3 Molding the powder to obtain a blank;
step C, placing the biscuit in a vacuum environment at 1200-1600 ℃ for sintering for 0.5-50h, and then heating in an inert gas at 1200-1600 ℃ and the likeStatic pressure sintering for 0.5-8h, annealing at 1100-1500 deg.C in air, oxygen or reducing atmosphere for 0.5-30h, and fine polishing two sides to obtain Cr, Y 2 O 3 A transparent ceramic.
As a preferred technical solution of the present invention, step a includes:
weighing Y 2 O 3 And a doping agent containing Cr is placed in a ball mill, and absolute ethyl alcohol is added to obtain mixed slurry;
adding grinding balls into the mixed slurry, and finishing the ball milling treatment of the slurry by a ball mill;
placing the mixed slurry subjected to ball milling treatment in an oven for drying to obtain a dried material;
grinding the dried material, and screening to obtain a screened material;
placing the obtained sieved material in a muffle furnace for calcination treatment to obtain Cr, Y 2 O 3 And (3) powder.
As a preferable technical scheme of the invention, the Cr-containing dopant is Cr 2 O 3 、CrCl 3 、Cr (NO 3 ) 3 、Cr 2 (SO 4 ) 3 One kind of (1).
As a preferred technical scheme of the invention, the absolute ethyl alcohol and the Y 2 O 3 And the volume ratio of the mixed powder containing the Cr dopant is 1;
and/or the rotating speed of the ball mill is 100-250 rpm, and the ball milling time is 3-48 h;
and/or the drying temperature of the mixed slurry is 40-120 ℃, and the drying time is 12-48h;
and/or the calcining temperature of the screened material is 600-1200 ℃, and the calcining time is 3-10h.
As a preferred embodiment of the present invention, the step B includes: mixing Cr with Y 2 O 3 Dry pressing the powder to form; to the dry-pressed Cr: Y 2 O 3 And carrying out cold isostatic pressing on the powder to obtain a biscuit.
As a preferred technical scheme of the invention, the pressure of the dry pressing molding is 5-20Mpa;
and/or the pressure of the cold isostatic pressing is 100-200Mpa.
As a preferred technical scheme of the invention, the vacuum degree of the vacuum environment is less than or equal to 10 -3 Pa。
In a preferred embodiment of the present invention, the pressure of the hot isostatic pressing sintering is 50 to 200MPa.
As a preferable technical scheme of the invention, the inert gas for hot isostatic pressing sintering is argon or/and nitrogen;
and/or the reducing atmosphere is hydrogen.
A nanocrystalline laser-grade sesquioxide transparent ceramic is prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, a proper amount of Cr is used as a dopant, so that the sintering temperature of pure sesquioxide ceramic can be reduced, and simultaneously, the prepared ceramic material can be ensured to have nano-scale grain size and laser-level transparency, and has excellent mechanical properties and infrared transmittance.
Drawings
FIG. 1 shows Cr: Y provided in examples 1 to 4 of the present invention 2 O 3 XRD of transparent ceramics.
FIG. 2 shows Cr: Y provided in examples 1 to 2 of the present invention 2 O 3 SEM after transparent ceramic hot isostatic pressing sintering.
FIG. 3 shows Cr: Y provided in example 12 of the present invention 2 O 3 And (3) a statistical graph of the grain size of the transparent ceramic after hot isostatic pressing sintering.
FIG. 4 shows Cr: Y provided in example 1 of the present invention 2 O 3 Infrared spectroscopy of transparent ceramics.
FIG. 5 is a process flow diagram of the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
As shown in figures 1 to 3, a method for preparing a nanocrystalline laser-grade sesquioxide transparent ceramic comprises the steps of A, mixing commercial high-purity Y 2 O 3 And a Cr-containing dopant as a raw material according to the chemical formula (Cr) x Y 1-x ) 2 O 3 Weighing and mixing to obtain mixed powder, wherein x is more than or equal to 0.0002 and less than or equal to 0.02, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Cr, Y 2 O 3 Powder;
the step A comprises the following steps:
weighing Y 2 O 3 And a doping agent containing Cr is placed in a ball mill, and absolute ethyl alcohol is added to obtain mixed slurry; absolute ethanol with Y 2 O 3 And the volume ratio of the mixed powder containing the Cr dopant is 1;
the Cr-containing dopant is preferably Cr 2 O 3 、CrCl 3 、Cr (NO 3 ) 3 、Cr 2 (SO 4 ) 3 One of them, also other Cr-containing dopants, can be determined according to actual requirements.
Adding grinding balls into the mixed slurry, and finishing ball milling treatment on the slurry through a ball mill; the rotating speed of the ball mill is 100-250 rpm, and the ball milling time is 3-48 h; the particle diameter of the powder after ball milling is 50-200nm.
Placing the mixed slurry subjected to ball milling treatment in an oven for drying to obtain a dried material; the drying temperature of the mixed slurry is 40-120 ℃, and the drying time is 12-48h.
Grinding and screening the dried material to obtain a screened material; the screening precision is between 80 and 300 meshes.
Placing the obtained sieved material in a muffle furnace for calcination treatment to obtain Cr, Y 2 O 3 Powder; the calcining temperature of the sieved materials is 600-1200 ℃, and the calcining time is 3-10h.
Step B, mixing Cr and Y 2 O 3 Molding the powder to obtain a blank;
Cr:Y 2 O 3 the powder is molded as follows: dry pressing to form and dry pressing to form Cr, Y 2 O 3 And carrying out cold isostatic pressing on the powder to obtain a blank.
The pressure of dry pressing is 5-20MPa, and the pressure of cold isostatic pressing is 100-200MPa.
Step C, placing the biscuit in a vacuum environment at 1200-1600 ℃ for sintering for 0.5-50h, wherein the vacuum degree of the vacuum environment is less than or equal to 10 -3 Pa；
Hot isostatic pressing sintering at 1200-1600 ℃ in inert gas for 0.5-8h, wherein the pressure of the hot isostatic pressing sintering is 50-200MPa, and the inert gas used for the hot isostatic pressing sintering is argon or/and nitrogen;
finally annealing for 0.5-30h in air, oxygen or reducing atmosphere at 1100-1500 ℃, wherein the oxidizing atmosphere for annealing is oxygen, and the reducing atmosphere is hydrogen or/and argon;
fine polishing on both sides to obtain Cr, Y 2 O 3 A transparent ceramic.
A nanocrystalline laser-grade sesquioxide transparent ceramic is prepared by the preparation method.
With Cr to Y 2 O 3 Ceramics are exemplified:
example one
(1) As commercial high purity Y 2 O 3 And Cr 2 O 3 Is used as raw material and has a chemical formula of 0.1 at.% Cr to Y 2 O 3 Weighing 100g of Y 2 O 3 Powder and 0.067g Cr 2 O 3 Pulverizing, adding anhydrous ethanol, and transferringBall milling is carried out for 24 h in a ball mill with the speed of 140 rpm. Then taking out the slurry, putting the slurry into a 70 ℃ oven for drying for 48h, grinding, sieving by a 140 mu m sieve, and finally putting the slurry into a 800 ℃ muffle furnace for calcining for 5 h to obtain Cr, Y 2 O 3 And (3) powder.
(2) Putting the powder into a mould, and carrying out dry pressing molding under the pressure of 10 MPa; then cold isostatic pressing was performed under a pressure of 200MPa.
(3) And (3) sintering the blank body in a vacuum environment at 1260 ℃ for 7 h, then performing hot isostatic pressing sintering in an argon atmosphere at 1240 ℃ for 3 h, and finally performing oxygen annealing in a tube furnace at 1100 ℃ for 20 h. Polishing two sides of the sample to obtain Cr, Y 2 O 3 A transparent ceramic.
Example two
(1) As commercial high purity Y 2 O 3 And Cr 2 O 3 Is used as raw material and has a chemical formula of 0.1 at.% Cr: Y 2 O 3 100g of Y are weighed 2 O 3 Powder and 0.067g Cr 2 O 3 Adding a proper amount of absolute ethyl alcohol into the powder, and then putting the mixture into a ball mill with the rotating speed of 140 rpm for ball milling for 24 hours. Then taking out the slurry, putting the slurry into a 70 ℃ oven for drying for 48h, grinding, sieving by a 140 mu m sieve, and finally putting the sieved powder into a 800 ℃ muffle furnace for calcining for 5 h to obtain Cr, Y 2 O 3 And (3) powder.
(2) Putting the powder into a mould, and carrying out dry pressing forming under the pressure of 10 MPa; then cold isostatic pressing was performed at a pressure of 200MPa.
(3) And (3) sintering the blank body in a vacuum environment at 1260 ℃ for 7 h, then performing hot isostatic pressing sintering in an argon atmosphere at 1240 ℃ for 3 h, and finally performing hydrogen annealing in a tube furnace at 1100 ℃ for 20 h. Polishing two sides of the sample to obtain Cr, Y 2 O 3 A transparent ceramic.
EXAMPLE III
(1) As commercial high purity Y 2 O 3 And Cr 2 O 3 Is used as raw material and has a chemical formula of 0.1 at.% Cr to Y 2 O 3 100g of Y are weighed 2 O 3 Powder and 0.067g Cr 2 O 3 Pulverizing, adding appropriate amount ofAfter the absolute ethyl alcohol is added, the mixture is put into a ball mill with the rotating speed of 140 rpm for ball milling for 24 hours. Then taking out the slurry, putting the slurry into a 70 ℃ oven for drying for 48h, grinding, sieving by a 140 mu m sieve, and finally putting the slurry into a 800 ℃ muffle furnace for calcining for 5 h to obtain Cr, Y 2 O 3 And (3) powder.
(2) Putting the powder into a mould, and carrying out dry pressing molding under the pressure of 10 MPa; then cold isostatic pressing was performed under a pressure of 200MPa.
(3) And (3) placing the blank body in a vacuum environment at 1330 ℃ for sintering for 7 h, then performing hot isostatic pressing sintering in an argon atmosphere at 1300 ℃ for 3 h, and finally performing oxygen annealing in a tube furnace at 1200 ℃ for 20 h. Polishing two sides of the sample to obtain Cr, Y 2 O 3 A transparent ceramic.
Example four
(1) As commercial high purity Y 2 O 3 And Cr 2 O 3 Is used as raw material and has a chemical formula of 0.1 at.% Cr to Y 2 O 3 Weighing 100g of Y 2 O 3 Powder and 0.067g Cr 2 O 3 Adding a proper amount of absolute ethyl alcohol into the powder, and then putting the mixture into a ball mill with the rotating speed of 140 rpm for ball milling for 24 hours. Then taking out the slurry, putting the slurry into a 70 ℃ oven for drying for 48h, grinding, sieving by a 140 mu m sieve, and finally putting the slurry into a 800 ℃ muffle furnace for calcining for 5 h to obtain Cr, Y 2 O 3 And (3) powder.
(2) Putting the powder into a mould, and carrying out dry pressing molding under the pressure of 10 MPa; then cold isostatic pressing was performed under a pressure of 200MPa.
(3) And (3) placing the blank body in a vacuum environment at 1330 ℃ for sintering for 7 h, then performing hot isostatic pressing sintering in an argon atmosphere at 1300 ℃ for 3 h, and finally performing hydrogen annealing in a tube furnace at 1200 ℃ for 20 h. Polishing two sides of the sample to obtain Cr, Y 2 O 3 A transparent ceramic.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a nanocrystalline laser-grade sesquioxide transparent ceramic is characterized by comprising the following steps:
step A, adding Y 2 O 3 And a Cr-containing dopant of the formula (Cr) x Y 1-x ) 2 O 3 Weighing and mixing to obtain mixed powder, wherein x is more than or equal to 0.0002 and less than or equal to 0.02, and performing ball milling, drying, grinding, sieving and calcining treatment in sequence to obtain Cr, Y 2 O 3 Powder;
step B, mixing Cr and Y 2 O 3 Molding the powder to obtain a blank;
step C, sintering the blank in a vacuum environment at 1200-1330 ℃ for 0.5-50h, sintering the blank in hot isostatic pressing in an inert gas at 1200-1300 ℃ for 0.5-8h, finally annealing the blank in air, oxygen or reducing atmosphere at 1100-1500 ℃ for 0.5-30h, and finely polishing the two sides to obtain Cr, Y 2 O 3 A transparent ceramic.
2. The method of claim 1, wherein step a comprises:
weighing Y 2 O 3 And a doping agent containing Cr is placed in a ball mill, and absolute ethyl alcohol is added to obtain mixed slurry;
adding grinding balls into the mixed slurry, and finishing ball milling treatment on the slurry through a ball mill;
placing the mixed slurry subjected to ball milling treatment in an oven for drying to obtain a dried material;
grinding the dried material, and screening to obtain a screened material;
placing the obtained sieved material in a muffle furnace for calcination treatment to obtain Cr, Y 2 O 3 And (3) powder.
3. The method of claim 2, wherein the nanocrystalline laser-grade sesquioxide transparent ceramic is prepared by the methodThe dopant containing Cr is Cr 2 O 3 、CrCl 3 、Cr (NO 3 ) 3 、Cr 2 (SO 4 ) 3 To (3) is provided.
4. The method of claim 2, wherein the absolute ethyl alcohol and Y are selected from the group consisting of 2 O 3 And the volume ratio of the mixed powder containing the Cr dopant is 1;
and/or the rotating speed of the ball mill is 100-250 rpm, and the ball milling time is 3-48 h;
and/or the drying temperature of the mixed slurry is 40-120 ℃, and the drying time is 12-48h;
and/or the calcining temperature of the screened material is 600-1200 ℃, and the calcining time is 3-10h.
5. The method of claim 1, wherein step B comprises: mixing Cr with Y 2 O 3 Dry pressing the powder to form; to the dry-pressed Cr: Y 2 O 3 And carrying out cold isostatic pressing on the powder to obtain a biscuit.
6. The method for preparing the nanocrystalline laser-grade sesquioxide transparent ceramic according to claim 5, wherein the pressure of the dry pressing is 5-20Mpa;
and/or the pressure of the cold isostatic pressing is 100-200Mpa.
7. The method of claim 1, wherein the vacuum degree of the vacuum environment is less than or equal to 10 -3 Pa。
8. The method of claim 1, wherein the hot isostatic pressing sintering is performed at a pressure of 50-200MPa.
9. The method of claim 1, wherein the inert gas used for hot isostatic pressing sintering is argon or/and nitrogen;
and/or the reducing atmosphere is hydrogen.
10. A nanocrystalline laser grade sesquioxide transparent ceramic prepared by the method of any one of claims 1 to 9.
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